CN105527391A - Electric-nose-analysis-based determination method of tuna oil corruption degree in storage process - Google Patents
Electric-nose-analysis-based determination method of tuna oil corruption degree in storage process Download PDFInfo
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Abstract
The present invention relates to an electric-nose-analysis-based determination method of tuna oil corruption degree in a storage process, according to the determination method, an electric-nose technology is used for research on volatile odor of tuna oil in the storage process, by principal component analysis (PCA) and linear discriminant analysis (LDA), fish oil samples of different storage time can be distinguished, and acid value and peroxide value forecast models can be established by partial least squares (PLS), so that the tuna oil corruption degree in the storage process can be effectively determined. Compared with the prior art, the determination method is simple in operation, short in detection time and high in detection efficiency, is a fast, effective and comprehensive determination of tuna oil quality, can be widely popularized in fish oil quality measurement.
Description
Technical field
The present invention relates to fish oil quality and measure field, particularly relate to a kind of assay method based on degree of spoilage in the tunny fish oil storage of Electronic Nose analysis.
Background technology
Electronic Nose is that do as one likes multiple chemical sensor that can overlap each other and suitable mode identification method form, and can identify the bionics instrument of simple and complicated smell.Be similar to the nose of humans and animals, the Global Information of what Electronic Nose " was smelt " is volatile ingredient in sample.During work, gas sensor array adsorbs gas, desorption or react, and produce electric signal, then leave that the signal that circuit and data acquisition system (DAS) produce sensor amplifies under order, A/D conversion, to gather and transmission, finally deliver to computing machine and pattern recognition system, pattern-recognition is carried out to signal, judge and Output rusults.Adopt the sample of Electronic Nose analysis not need pre-service, detection speed is fast, and each sample only needs tens seconds, simultaneously again can the overall odiferous information of representative sample.
Tunny fish oil is rich in polyunsaturated fatty acid EPA and DHA, have good health-care effect, but EPA and DHA is very easily oxidized to human body, causes fish oil quality to decline.At present, evaluate fish oil quality mainly to be measured by the chemical index such as acid value, peroxide value and subjective appreciation, gas chromatograph-mass spectrometer (GCMS) (GC-MS) coupling technique analysis volatile constituent etc.Subjective appreciation poor accuracy, evaluation result varies with each individual, and steel used in tank technical costs is high, analysis time is long, and test result is the result of sample after being separated substantially, is difficult to the globality of representative sample.
In recent years, Electronic Nose Technology was used widely at field of food, studies have reported that, but the research that Electronic Nose is applied to fish oil quality had no report at home in the fields such as fruits and vegetables class, grain and oil class, meat poultry, beverage.
Summary of the invention
Technical matters to be solved by this invention provides a kind of fast and effectively based on the assay method of degree of spoilage in the tunny fish oil storage of Electronic Nose analysis.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of assay method based on degree of spoilage in the tunny fish oil storage of Electronic Nose analysis, is characterized in that comprising the following steps:
(1) mensuration of physical and chemical index
Measure acid value and the peroxide value of modeling standard tunny fish oil respectively, every 5d measures once;
(2) Electronic Nose measures
Modeling standard tunny fish oil is put into airtight container, 25 ~ 30min is left standstill in 20 ~ 25 DEG C of water-baths, use the gas in the sample introduction needle aspirate airtight container of Electronic Nose at normal temperatures, the absorption time is 30 ~ 60s, the gas sensor array of gas in Electronic Nose device detects, this gas sensor array is by fragrance ingredient sensor W1C, nitrogen oxide sensor W5S, ammonia gas sensor W3C, hydrogen gas sensor W6S, alkane fragrance ingredient sensor W5C, methane transducer W1S, sulfide sensor W1W, ethanol sensor W2S, organic sulfide sensor W2W and alkane sensor W3S forms,
(3) foundation of acid value and peroxide value forecast model
Collect the data that gas sensor array gathers, carry out principal component analysis (PCA), linear discriminant analysis and Load Analysis, wherein the validity of principal component analysis (PCA) is with first principal component and the total contribution rate 90% of Second principal component, for threshold values, if total contribution rate is less than this threshold values, revises the detected parameters of Electronic Nose until total contribution rate is more than or equal to this threshold values;
Partial least square method is utilized comprehensively to analyze the physical and chemical index data gathered and Electronic Nose test data and build acid value and peroxide value forecast model respectively, with acid value and peroxide value predicted value for ordinate, Electronic Nose actual measurement is horizontal ordinate, sets up acid value PLS linear fit curve and peroxide value PLS linear fit curve respectively;
(4) Electronic Nose is utilized to gather the data of tunny fish oil to be measured, by these data by above-mentioned steps 3) model that obtains analyzes, obtains acid value and peroxide value prediction, thus measure degree of spoilage in tunny fish oil storage.
First principal component mainly reflects oxynitrides, the contribution rate of sensor W5S to first principal component is maximum, what Second principal component, mainly reflected is fragrance ingredient, ethanol, sulfide and methane content, the contribution rate of sensor W2W to Second principal component, is maximum, sensor W2S, the contribution rate of W1W and W1S to Second principal component, is larger, consider the contribution rate of Second principal component, contribution rate far below first principal component, i.e. sensor W2W, W2S, W1W and W1S can ignore on the impact of tunny fish oil smell, therefore in the present invention according to SC/T3502-2000 rower crude fish oil secondary standard (acid value≤15mgKOH/kg, peroxide value≤10mmol/kg), according to Electronic Nose response, using W5S as the most responsive sensor, its G/G0 is Acid value over national standard in 43 ~ 52 scopes, G/G0 exceeds standard in 20 ~ 30 scope endoperoxides values, wherein, G/G0 is the response that Electronic Nose exports, it is according to the resistance G after sensor contacts to sample volatile matter and the sensor ratio at the resistance G0 through standard activity charcoal filtering gas.
As preferably, in described step (3), the regression equation of acid value PLS linear fit curve is: Y=1.02986X-0.48431, R
2=0.9415, the regression equation of peroxide value linear fit curve is: Y=0.96907X+0.26401, R
2=0.9846.
As preferably, GB GB/T5530-2005 and GB/T5538-2005 in described step (1), is adopted to measure acid value and the peroxide value of modeling standard tunny fish oil respectively.
Described step (2) Electronic Nose test condition is: carrier gas flux is 300mL/min, and sensor scavenging period is 60s, and sampling time interval is 1s, and gas sampling flow is 300mL/min, and acquisition time is 70s.
Compared with prior art, the invention has the advantages that: the present invention is studied the volatile flavor of tunny fish oil in storage by Electronic Nose Technology, use principal component analysis (PCA) (PCA), the fish oil sample of different storage time is distinguished in linear discriminant analysis (LDA), and set up acid value by partial least square method (PLS), the forecast model of peroxide value, thus tunny fish oil degree of spoilage in storage is effectively measured, simple to operate, detection time is short, detection efficiency is high, fast a kind of, effectively, comprehensive tunny fish oil quality determination method, can extensively be extended in the mensuration of fish oil quality.
Accompanying drawing explanation
Fig. 1 is the 59s radar map of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention;
Fig. 2 is the PCA figure of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention;
Fig. 3 is the LDA figure of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention;
Fig. 4 is the loading analysis figure of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention;
Fig. 5 is the acid value PLS analysis chart of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention;
Fig. 6 is the peroxide value PLS analysis chart of the modeling standard gold marlin oil samples of different storage time in the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
One, the foundation of tunny fish oil acid value and peroxide value forecast model
1, test method
1.1 physical and chemical indexs measure
Acid value, peroxide value adopt national standard method GB/T5530-2005, GB/T5538-2005 to measure respectively, and every 5d measures once.
1.2 Electronic Nose assay methods
Get modeling standard gold marlin oil samples 1g (accurately to 0.01g), put into 10mL ml headspace bottle, seal, balance 30min in 25 DEG C of water-baths, adopt Electronic Nose head space Direct Analysis, carrier gas flux 300mL/min, gas sampling flow 300mL/min, sensor scavenging period 60s, sampling time interval 1s, the test duration is 70s.Sample measures once every 5d.PEN3 type portable Electronic Nose comprises 10 metal oxide sensor arrays, and the title of each sensor and performance describe in table 1.Above-mentioned modeling standard gold marlin oil samples used is provided by Zhejiang Feng Yu biological products company limited, the cooking liquor oil and water separation produced through wet pressing technique tuna powder obtains, wherein moisture 0.23%, unsaponifiables 0.91%, acid value 10.33mgKOH/g, peroxide value 7.97mmol/kg, iodine number 181.6gI/100g, keep in Dark Place at 25 DEG C; It is pure that potassium iodide used, NaOH, methenyl choloride, glacial acetic acid, ether, ethanol etc. are analysis.
Table 1 Electronic Nose sensor performance describes
1.3 data processing
Data processing and the mapping of acid value, peroxide value adopt Origin8.5 software; The Winmuster data vector program that Electronic Nose data processing adopts PEN3 electric nasus system to carry, multivariate statistical analysis is carried out to collection volatile flavor information, comprises principal component analysis (PCA) (PCA), linear discriminant analysis (LDA), loading analysis (Loadings) and partial least square method (PLS).
2, test findings
The 2.1 different storage time tunny fish oil index of quality
The physical and chemical index that fish oil measures mainly comprises acid value, peroxide value, iodine value, unsaponifiables, moisture etc., can reflect fish oil quality.Table 2 is the measured value of acid value and peroxide value in storage, the hydrolytic process in this two indices and storage and oxidizing process product closely related.As can be seen from Table 1, compared with storage 0d, the acid value of fish oil and peroxide value all have the change (P < 0.05) of conspicuousness with the prolongation of storage time, wherein, when storage time is 10d, 15d, 20d, the data variation of acid value, peroxide value is little, and there is of short duration drop at 20d in acid value, but there was no significant difference, and peroxide value is at 10d, 15d also there was no significant difference.After 25d, acid value, peroxide value amplification become large, and significant difference is obvious, and aggravation of becoming sour is described, fish oil quality declines obviously.
Acid value and peroxide value change in table 2 storage
Note: lowercase difference in the same column data upper right corner represents significant difference (P < 0.05).
The tunny fish oil fingerprint characteristic of 2.2 different storage times is analyzed
Compared to the delta data of sensor, Electronic Nose radar map can observe the difference of different storage time lower sensor response signal more intuitively.As seen from Figure 1, the reaction signal intensity of tunny fish oil sample to Electronic Nose 10 sensors of different storage time is variant, storage time is longer, the response of sensor is increasing, in radar map, the region of lower display is also larger, namely the volatile flavor in tunny fish oil sample gets more and more, and wherein the response of sensor W5S is maximum, is secondly sensor W2W.Therefore, the different tunny fish oil sample of storage time can obviously be distinguished by radar map.
2.3, principal component analysis (PCA) (PCA)
As seen from Figure 2, first principal component and Second principal component, contribution rate are respectively 99.31% and 0.31%, and total contribution rate is 99.62%, illustrate that major component can reflect the characteristic information of different storage time tunny fish oil sample volatile flavor preferably.Storage 0,5, there is overlap in the sample smell region of 10d, volatile ingredient has certain general character, illustrates that tunny fish oil sample volatile ingredient in front 10d changes not obvious, may be the slow cause of oxidative rancidity speed; Though the zero lap district, sample smell region of storage 15,20d, its horizontal ordinate range difference, apart from little, is difficult to make a distinction; 25,30,35d smell region separates successively with abscissa axis direction, and the volatile flavor of interpret sample is showed increased with the prolongation of storage time, may be repeatedly sample oxygen repeatedly to enter the cause making oil sample be oxidized aggravation.Tunny fish oil is difficult to separately in 10d, 15d, 20d flavor region at horizontal ordinate, namely major component change is little, after 25d, tunny fish oil flavor region increases with storage time and arranges successively on the horizontal scale, and illustrate that smell increases obviously, this conforms to substantially with 2.1 analysis results.
2.4 linear discriminant analysiss (LDA)
As seen from Figure 3, first principal component contribution rate is 59.94%, and Second principal component, contribution rate is 19.09%, and total contribution rate is 79.03%, illustrates that discriminatory analysis result can represent most of odiferous information.Except the storage time sample smell region that is 5d and 10d overlaps, other equal zero laps in smell region.On the tunny fish oil sample Second principal component, of storage 30d and 35d, difference is little, but according to the span of each smell region on abscissa axis in Fig. 3, the sample of storage different time can make a distinction completely.Comparison diagram 2 and Fig. 3 known, although total LDA method contribution rate is lower than the total contribution rate of PCA method, but distinguish effect be much better than PCA method.
2.5 loading analyses (Loadings)
As shown in Figure 4,10 kinds of sensors are to the sensitivity of the tunny fish oil of storage different time, judge its power to tunny fish oil odor identification ability according to sensor response, the contribution rate of sensor W5S to first principal component is maximum, illustrates that first principal component mainly reflects oxynitrides; The contribution rate of sensor W2W to Second principal component, is maximum, and sensor W2S, W1W and W1S are comparatively large to the contribution rate of Second principal component, and what describe that Second principal component, mainly reflects is fragrance ingredient, ethanol, sulfide and methane content.Consider the contribution rate of Second principal component, contribution rate far below first principal component, namely sensor W2W, W2S, W1W and W1S can ignore on the impact of tunny fish oil smell.Sensor W1C, W3C, W5C, W6S, W3S distribution is more close, and all close to (0,0), illustrate that signal is more weak, contribution rate is less, therefore it is very weak to the sensitivity of tunny fish oil smell, can ignore.It can thus be appreciated that oxynitrides is the volatile ingredient larger to tunny fish oil odor impact, this may with tunny fish oil in storage, and the product that the factor such as light, oxygen causes it that oxidative rancidity constantly occurs is relevant.
The foundation of 2.6 tunny fish oil acid values and peroxide value forecast model
Adopt partial least square method (PLS) analyze tunny fish oil smell and quality comparison in storage and build forecast model, respectively with acid value and peroxide value predicted value for ordinate, Electronic Nose actual measurement is horizontal ordinate, sets up PLS linear fit curve.Fig. 5, Fig. 6 are the PLS analysis chart of acid value, peroxide value respectively.
From the regression equation of Fig. 5 and Fig. 6, PLS acid number typical curve be: Y=1.02986X-0.48431, R
2=0.9415; The regression equation of PLS peroxide value typical curve is: Y=0.96907X+0.26401, R
2=0.9846.Illustrate tunny fish oil in storage acid value, between peroxide value and Electronic Nose sensor signal, there is good linear relationship.
Further, according to SC/T3502-2000 rower crude fish oil secondary standard (acid value≤15mgKOH/kg in the present invention, peroxide value≤10mmol/kg), according to Electronic Nose response, using W5S as the most responsive sensor, its G/G0 is Acid value over national standard in 43 ~ 52 scopes, and G/G0 exceeds standard in 20 ~ 30 scope endoperoxides values.
Two, the checking of forecast model
For checking, institute sets up the accuracy of forecast model, measures tunny fish oil (production of Zhejiang Feng Yu biological products company limited) acid value, the peroxide value of 5 groups of different storage times, and do Electronic Nose simultaneously and test, comparison prediction value and measured value, the results are shown in Table 3.Obtain acid value predicted value and measured value mean relative deviation is 10.60%, peroxide value predicted value and measured value mean relative deviation are 12.04%, and known built forecast model can be used for predicting acid value, peroxide value.
Table 3 acid value, peroxide value forecast model confirmatory experiment
Claims (4)
1., based on an assay method for degree of spoilage in the tunny fish oil storage of Electronic Nose analysis, it is characterized in that comprising the following steps:
(1) mensuration of physical and chemical index
Measure acid value and the peroxide value of modeling standard tunny fish oil respectively, every 5d measures once;
(2) Electronic Nose measures
Modeling standard tunny fish oil is put into airtight container, 25 ~ 30min is left standstill in 20 ~ 25 DEG C of water-baths, use the gas in the sample introduction needle aspirate airtight container of Electronic Nose at normal temperatures, the absorption time is 30 ~ 60s, the gas sensor array of gas in Electronic Nose device detects, this gas sensor array is by fragrance ingredient sensor W1C, nitrogen oxide sensor W5S, ammonia gas sensor W3C, hydrogen gas sensor W6S, alkane fragrance ingredient sensor W5C, methane transducer W1S, sulfide sensor W1W, ethanol sensor W2S, organic sulfide sensor W2W and alkane sensor W3S forms,
(3) foundation of acid value and peroxide value forecast model
Collect the data that gas sensor array gathers, carry out principal component analysis (PCA), linear discriminant analysis and Load Analysis, wherein the validity of principal component analysis (PCA) is with first principal component and the total contribution rate 90% of Second principal component, for threshold values, if total contribution rate is less than this threshold values, revises the detected parameters of Electronic Nose until total contribution rate is more than or equal to this threshold values;
Partial least square method is utilized comprehensively to analyze the physical and chemical index data gathered and Electronic Nose test data and build acid value and peroxide value forecast model respectively, with acid value and peroxide value predicted value for ordinate, Electronic Nose actual measurement is horizontal ordinate, sets up acid value PLS linear fit curve and peroxide value linear fit curve respectively;
(4) utilize Electronic Nose to gather the data of tunny fish oil to be measured, the model that these data are obtained by above-mentioned steps (3) is analyzed, obtain acid value and peroxide value prediction, thus measure degree of spoilage in tunny fish oil storage.
2. assay method as claimed in claim 1, is characterized in that, in described step (3), the regression equation of acid value PLS linear fit curve is: Y=1.02986X-0.48431, R
2=0.9415, the regression equation of peroxide value linear fit curve is: Y=0.96907X+0.26401, R
2=0.9846.
3. assay method as claimed in claim 1, is characterized in that, adopts GB GB/T5530-2005 and GB/T5538-2005 to measure acid value and the peroxide value of modeling standard tunny fish oil in described step (1) respectively.
4. assay method as claimed in claim 1, it is characterized in that, described step (2) Electronic Nose test condition is: carrier gas flux is 300mL/min, sensor scavenging period is 60s, sampling time interval is 1s, and gas sampling flow is 300mL/min, and acquisition time is 70s.
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| CN110726755A (en) * | 2019-11-05 | 2020-01-24 | 贺州学院 | Steamed Lipu taro quality discrimination method based on sensory evaluation and electronic nose analysis |
| CN112326625A (en) * | 2020-11-06 | 2021-02-05 | 四川省丹丹郫县豆瓣集团股份有限公司 | Finished product detection method for improving food safety prevention and control level |
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Application publication date: 20160427 |